EP1829843B1 - Appareil pour traiter des pieces poreuses en carbone - Google Patents

Appareil pour traiter des pieces poreuses en carbone Download PDF

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Publication number
EP1829843B1
EP1829843B1 EP06026557.6A EP06026557A EP1829843B1 EP 1829843 B1 EP1829843 B1 EP 1829843B1 EP 06026557 A EP06026557 A EP 06026557A EP 1829843 B1 EP1829843 B1 EP 1829843B1
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Prior art keywords
chamber
workpieces
workpiece
silicon
chambers
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German (de)
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EP1829843A3 (fr
EP1829843A2 (fr
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Andreas Kienzle
Johann Daimer
Rudi Beck
Otto Mederle
Matthieu Schwartz
Jens Rosenlöcher
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Audi AG
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Audi AG
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    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/02—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity of multiple-track type; of multiple-chamber type; Combinations of furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/04—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity adapted for treating the charge in vacuum or special atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
    • F27B9/20—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/30—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B9/36—Arrangements of heating devices
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
    • C04B2235/662—Annealing after sintering
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Definitions

  • the present invention relates to a device for siliconising carbonaceous materials.
  • a method for producing a silicon-impregnated body of silicon carbide in which a mixture of silicon carbide powder with graphite powder and a silicone resin is granulated, compacted and calcined at about 800 ° C. The calcined body is heated under reduced pressure to 1500 ° C and impregnated with molten silicon. The thus prepared body is then sintered at 1600 ° C to 1800 ° C.
  • EP 0 453 592 discloses a method of making siliconized silicon carbide articles by first injecting an injection molded body of silicon carbide particles and an organic binder into a porous body containing silicon carbide and elemental carbon, which is subsequently infiltrated with molten silicon, by heating; wherein the elemental carbon is converted to silicon carbide.
  • the sprue of the injection-molded body is used as a feed for the molten silicon.
  • the patent application EP 1 607 704 A1 relates to a continuously operated furnace for burning tiles or for tempering pressed steel parts.
  • the patent application DE 197 10 105 A1 relates to a silicon carbide body reinforced with graphite short fibers, and a process for the production thereof, in which the body to be silicided, which must have an open pore system penetrating the whole body, is placed in a container, on the bottom of which is molten silicon. See page 4, line 67, to page 5, line 1.
  • the bodies which are to be silicided are porous carbon bodies which are very absorbent in relation to the silicon and whose lower part is in liquid silicon. The silicon then passes through these wick bodies into the bodies to be silicided without the latter having direct contact with the silicon bath. See page 5, lines 29 to 31.
  • a furnace at the bottom of which is a well with silicon, in the three columnar supports made of highly porous CFC material (with fibers of Carbon reinforced carbon) are arranged as wicks on which the body to be silicided is applied.
  • the furnace is pumped to a pressure of 3 hPa (3 mbar) and heated to a temperature of 1750 ° C within two hours, maintained at this temperature for a further ten minutes at 1750 ° C, and then cooled.
  • step b the pressure is lowered to the operating pressure p B 1 after or before heating or during heating, but always after the step of purging with inert gas.
  • the device according to the invention consists of at least four chambers O1 to O4 which are interconnected by locks, each of the chambers being heatable, coolable, evacuatable and to be filled or flushed with suitable gases independently of their neighbors.
  • each of the chambers O i is provided with at least one transport or conveyor, by means of which the workpieces are transported from the previous chamber O i-1 into the chamber O i and out of the chamber O i into the following chamber O i + 1
  • the index i can assume the values 1, 2, 3 and 4.
  • the device according to the invention allows the spatial separation of the individual process steps and a tact-like semi-continuous promotion of workpieces in separate chambers by locks and the environment, this gives rise to the possibility of the operating state (temperature, pressure) in the individual chambers as constant as possible; this leads to uniform operating states, reduction of energy requirements, and higher flexibility in production.
  • the conveyance or transport of the workpieces can be done by known means and methods, for example by sliding or conveying by means of a slider, by transport on rollers, by means of one or more lifting bars, or on a link chain.
  • materials are used for the transport, which withstand the selected temperatures and the media used, for example, selected from graphite and other carbon materials, the fibers z.
  • the steps a and b and the steps d and e can each be carried out in a common chamber, while otherwise at least one separate chamber is provided for each of the method steps.
  • the heating in the chambers is done with known heaters, especially infrared heaters, inductive heaters, microwave heating and heating by warmed gas (inert gas).
  • the cooling is carried out by flowing through the relevant chamber with a cooled gas stream, with inert gases such as nitrogen and argon are preferred at higher temperatures, while at temperatures of at most 300 ° C and air can be used.
  • induction heating in the chamber O1 , since this type of heating can very quickly introduce large amounts of energy into the workpiece.
  • a flushed with an inert gas preferably with nitrogen or argon
  • an induction heater 11 from room temperature to the operating temperature T B 1 heated, which may be from 1300 ° C to 1800 ° C, preferably 1350 ° C to 1750 ° C.
  • the operating pressure of 1 bar is lowered to a value p B 1 of at most 100 mbar (100 hPa), more preferably up to 50 hPa (50 mbar), and in particular at most 20 mbar (20 hPa) .
  • p B 1 of at most 100 mbar (100 hPa), more preferably up to 50 hPa (50 mbar), and in particular at most 20 mbar (20 hPa) .
  • a negative pressure is generated in the chamber O1 , as he also preferably constantly prevails in the chamber O2 , of at most 1 Pa (10 -2 mbar).
  • this pressure is reached, the workpiece is transported through the lock 20 into the chamber O2 , where it is now referred to as 95 .
  • a new workpiece is introduced from outside through the lock 10 into the chamber O1 and heated as described above.
  • the workpiece 95 is received at an operating pressure p B 2 of at most 10 -2 mbar (1 Pa) and at an adjustable via the heater 21 operating temperature T B 2 of 1450 ° C to 1700 ° C by a transport device, not shown and placed on the pads (porous wicks) 26 placed in the siliconizer 27 .
  • this siliconizing device 27 according to method step c, liquid silicon 25 located in a basin 22 passes via the porous wicks 26 into the workpiece 95 made of carbon.
  • silicon penetrates into the pores of the workpiece 95 and reacts, at least in part, according to process step d with the carbon present in the workpiece to silicon carbide.
  • the workpiece is called a "siliconized workpiece" after this treatment.
  • the basin 22 in the chamber O2 becomes one or more (in the drawing Fig. 2a in the number of two shown) pressure cells 28 ; this makes it possible to determine the mass of the silicon absorbed in the workpiece by weighing the basin before placing the workpiece 95 and after infiltration and removing the workpiece 95 .
  • the siliconized workpiece 95 is lifted off the wicks and transported through the sheath 30 into the chamber O3 .
  • the level of liquid silicon in the basin 22 is restored to the preset value after each cycle (extension of a siliconized workpiece 95 from O2 and inlet of a fresh preheated workpiece from the chamber O1 ) to a liquid silicon reservoir 23 passing through a pipe 24 is connected to the basin 22 .
  • the reaction according to the process step d in the siliconized workpiece is completed to the desired extent, whereby the spatial separation from the chamber O2 affords the favorable possibility, at a temperature T B 3, which is at least 50 K above the temperature T B 2, to anneal the workpiece in the chamber O3 without running the risk that escapes from the tank 22 as in the election of a higher temperature in the chamber O2 due to the higher vapor pressure of silicon.
  • T B 3 which is at least 50 K above the temperature T B 2
  • the temperature range for such a post-reaction is from 1500 ° C to 1900 ° C, more preferably from 1600 ° C to 1900 ° C, and especially from 1700 ° C to 1800 ° C.
  • the formation of silicon carbide can thus proceed much faster, leading to a desirable shortening of the cycle times in the process.
  • the heating in the chambers O2 and O3 is preferably carried out by radiant heating, for example, brought by Joule'sche heat annealed graphite heaters 21 and 31.
  • the workpiece in the chamber O3 by blowing cold inert gas according to the method step e cooled to a conditioning temperature T K in the range of 500 ° C to 300 ° C.
  • the workpiece 96 is brought through the lock 40 in the chamber O4 and there in the position 97 according to the method step f further first with inert gas, cooled from temperatures of at most 300 ° C and with air to room temperature. Through the lock 50 then the finished workpiece 98 can be discharged. Of course, before the next workpiece 95 is transferred into the chamber O3 for post-reaction, this chamber O3 is evacuated back to the operating pressure p B 3.
  • a residence time of the workpieces in the chambers O1 to O4 of three minutes to twenty minutes has been found to be favorable.
  • the process ensures that the workpieces 95 placed in the O2 chamber are always brought to the operating temperature prevailing in O2 , and that the operating pressure in O2 is always maintained.
  • This uniformity of pressure and temperature in the siliconizing step has proven to be essential for achieving consistent product quality.
  • a further advantage is that the workpieces are not cooled in contact with the silicon bath, thereby avoiding that pores formed by volume contraction of the silicon upon cooling are filled by post-sucked silicon. If several process steps are carried out in one of the chambers, for example in the step of post-reaction O3, optionally at elevated temperature compared to O2 takes place, and then the cooling, it is further preferred to divide these chambers.
  • the workpieces may have molded nipples 201 on a flat side, these nipples 201 having a constriction towards this flat side, as shown in FIG Fig. 2b and enlarged in the Fig. 2c is shown.
  • These nipples 201 submerge in the liquid silicon 25 in the silicon bath 27 , or stand on the supports 29. After removal of the finished workpieces from the device, these nipples 201 are easily broken off, since the extent of constriction is chosen such that in order to make this possible.
  • alloys or liquid mixtures of silicon with one or more other elements for infiltration.
  • additions of iron in a proportion by mass of up to 6% in the mixture
  • refractory metals such as chromium, molybdenum, tungsten, zirconium (in a proportion by mass of up to 3% in the mixture) as well as manganese, aluminum, Cobalt and nickel (in a proportion by mass of up to 3% in the mixture) proved.

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  • Mechanical Engineering (AREA)
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Claims (5)

  1. Dispositif de traitement de pièces en carbone poreux avec du silicium liquide avec formation de carbure de silicium, constitué d'au moins quatre chambres (O1, O2, O3 et O4) qui peuvent être séparément chauffées, refroidies, vidées et remplies avec des gaz et qui sont reliées les unes aux autres par des vannes,
    dans lequel, dans une forme de réalisation avec quatre chambres, il est prévu à chaque fois une chambre pour les étapes de procédé c et f et à chaque fois une chambre pour les étapes de procédé a et b ainsi que d et e à mettre en oeuvre l'une après l'autre à chaque fois à l'intérieur,
    dans lequel les étapes sont définies comme suit
    a préchauffage de pièces en carbone poreux dans une atmosphère de gaz inerte à la température de service choisie TB1 dans la chambre O1 dans une plage allant de 1 300 °C à 1 800 °C, par introduction des pièces dans la première chambre O1, rinçage de la chambre après la fermeture de la vanne avec un jet de gaz inerte et chauffage de la température ambiante à la température de service TB1,
    b diminution de la pression dans la chambre O1 au plus tard avant l'ouverture de la vanne 20 vers la chambre O2 à la pression de service inférieure à 10 hPa,
    c amenée du silicium liquide aux pièces de carbone poreux qui ont été reçues par un dispositif de transport dans la chambre O2 et posées sur les supports 26, agencés dans le dispositif d'imprégnation de silicium et réalisés sous forme de mèches poreuses, à une pression de service pB2 dans la chambre O2 de 1 Pa au maximum et à une température de service TB2 dans la chambre O2 dans une plage allant de 1450 °C à 1700 °C, et imprégnation des pièces en carbone poreux avec du silicium liquide, le silicium réagissant au moins partiellement avec le carbone présent dans la pièce pour former du carbure de silicium, avec formation d'une pièce imprégnée de silicium,
    d soulèvement des pièces imprégnées de silicium des mèches 26 et transport des pièces imprégnées de silicium via la vanne 30 dans la chambre O3, réaction du silicium liquide dans les pièces à une température TB3 dans la chambre O3 dans une plage allant de 1 500 °C à 1 900 °C, la température de service TB3 dans la chambre O3 étant supérieure d'au moins 50 K à la température de service TB2 avec formation de carbure de silicium à partir du carbone et du silicium,
    e gazage de la pièce dans la chambre O3 par insufflation de gaz inerte froid et refroidissement de la température de service TB3 à une température de conditionnement Tk dans une plage allant de 500 °C à 300 °C, la pression augmentant de moins de 1 hPa initialement à la pression normale de 105 Pa,
    f transport des pièces 96 via la vanne 40 dans la chambre O4, et refroidissement des pièces dans la position 97 à la température ambiante, d'abord avec du gaz inerte et à partir de températures de 300 °C au maximum également avec de l'air, et retrait des pièces fabriquées 98 via la vanne 50,
    dans lequel il est prévu dans la chambre O2 pour l'étape de procédé c un dispositif d'imprégnation de silicium qui comprend un bassin avec du silicium liquide et des supports réalisés sous forme de mèches poreuses pour la pièce
    et dans lequel la température TB3 est supérieure d'au moins 50 K à la température de service TB2, et la pièce dans la chambre O3 pour l'étape de procédé d n'est plus en contact avec le silicium liquide en dehors de la pièce.
  2. Dispositif selon la revendication 1 avec cinq chambres qui peuvent être séparément chauffées, refroidies, vidées et remplies avec des gaz et qui sont reliées les unes aux autres par des vannes, dans lequel des chambres séparées sont prévues à chaque fois pour les étapes de procédé d et e.
  3. Dispositif selon la revendication 1 avec cinq chambres qui peuvent être séparément chauffées, refroidies, vidées et remplies avec des gaz et qui sont reliées les unes aux autres par des vannes, dans lequel des chambres séparées sont prévues à chaque fois pour les étapes de procédé a et b.
  4. Dispositif selon la revendication 1 avec six chambres qui peuvent être séparément chauffées, refroidies, vidées et remplies avec des gaz et qui sont reliées les unes aux autres par des vannes, dans lequel des chambres séparées sont prévues à chaque fois pour les étapes de procédé a et b et pour les étapes de procédé d et e.
  5. Dispositif selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'il est prévu à chaque fois au moins deux chambres pour au moins l'une des étapes a à f.
EP06026557.6A 2006-03-01 2006-12-21 Appareil pour traiter des pieces poreuses en carbone Active EP1829843B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102006009388A DE102006009388B4 (de) 2006-03-01 2006-03-01 Vorrichtung zur Silicierung von kohlenstoffhaltigen Werkstoffen und darin durchführbares Verfahren

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EP1829843A2 EP1829843A2 (fr) 2007-09-05
EP1829843A3 EP1829843A3 (fr) 2008-07-02
EP1829843B1 true EP1829843B1 (fr) 2018-06-27

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Also Published As

Publication number Publication date
US7763224B2 (en) 2010-07-27
DE102006009388B4 (de) 2009-02-26
DE102006009388A1 (de) 2007-09-06
US20080213155A1 (en) 2008-09-04
EP1829843A3 (fr) 2008-07-02
US9663406B2 (en) 2017-05-30
US20100043699A1 (en) 2010-02-25
EP1829843A2 (fr) 2007-09-05

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